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INTERNATIONAL ISO
STANDARD 976

Fourth edition
2013-12-01

Rubber and plastics — Polymer

dispersions and rubber latices —
Determination of pH
Caoutchouc et plastiques — Dispersions de polymères et latex de
caoutchouc — Détermination du pH

Reference number
ISO 976:2013(E)

© ISO 2013
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ISO 976:2013(E)


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ISO 976:2013(E)


Contents Page

Foreword......................................................................................................................................................................................................................................... iv
1 Scope.................................................................................................................................................................................................................................. 1
2 Normative references....................................................................................................................................................................................... 1
3 Reagents......................................................................................................................................................................................................................... 1
4 Apparatus...................................................................................................................................................................................................................... 2
5 Sampling......................................................................................................................................................................................................................... 2
6 Procedure..................................................................................................................................................................................................................... 2
6.1 General............................................................................................................................................................................................................ 2
6.2 Maintenance of the electrode...................................................................................................................................................... 3
6.3 Calibration of the pH-meter.......................................................................................................................................................... 4
6.4 Measurement of the pH of the test sample...................................................................................................................... 5
7 Expression of results......................................................................................................................................................................................... 6
8 Test report.................................................................................................................................................................................................................... 6
Annex A (informative) Precision................................................................................................................................................................................ 7
Bibliography................................................................................................................................................................................................................................. 9

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ISO 976:2013(E)


Foreword
ISO (the International Organization for Standardization) is a worldwide federation of national standards
bodies (ISO member bodies). The work of preparing International Standards is normally carried out
through ISO technical committees. Each member body interested in a subject for which a technical
committee has been established has the right to be represented on that committee. International
organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.
ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of
electrotechnical standardization.
The procedures used to develop this document and those intended for its further maintenance are
described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the
different types of ISO documents should be noted. This document was drafted in accordance with the
editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of
any patent rights identified during the development of the document will be in the Introduction and/or
on the ISO list of patent declarations received (see www.iso.org/patents).
Any trade name used in this document is information given for the convenience of users and does not
constitute an endorsement.
For an explanation on the meaning of ISO specific terms and expressions related to conformity
assessment, as well as information about ISO’s adherence to the WTO principles in the Technical Barriers
to Trade (TBT) see the following URL: Foreword - Supplementary information
The committee responsible for this document is ISO/TC 45, Rubber and rubber products, Subcommittee
SC 3, Raw materials (including latex) for use in the rubber industry.
This fourth edition cancels and replaces the third edition (ISO 976:1996), which has been technically revised.
It also incorporates the Amendment (ISO 976:1996/Amd.1:2006). The following are the main changes:
— the normative references were updated;
— in (subclause) 4.2, the contact details of a provider of combined electrodes were deleted;
— the precision data were updated.

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INTERNATIONAL STANDARD ISO 976:2013(E)

Rubber and plastics — Polymer dispersions and rubber

latices — Determination of pH
WARNING — Persons using this International Standard should be familiar with normal laboratory
practice. This International Standard does not purport to address all of the safety problems, if
any, associated with its use. It is the responsibility of the user to establish appropriate safety and
health practices and to ensure compliance with any national regulatory conditions.

1 Scope
This International Standard specifies a method for the determination of the pH of polymer dispersions
and rubber latices (natural and synthetic) by means of a pH-meter equipped with a combined glass and
silver reference electrode.
The method is also suitable for prevulcanized latex and compounds containing polymer dispersions or
rubber latices, including adhesives.
NOTE The accuracy of the method decreases at pH values above 11.

2 Normative references
The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.
ISO 123, Rubber latex — Sampling
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 15528, Paints, varnishes and raw materials for paints and varnishes — Sampling

3 Reagents
Use commercially available analytical-grade buffer solutions of known pH or, in the absence of
commercial buffer solutions, prepare the solutions required (3.1, 3.2 and 3.3) using only reagents of
recognized analytical grade and carbon dioxide-free distilled water or water of equivalent purity (grade
3 as defined in ISO 3696).

3.1 Buffer solution, of nominal pH 7.

Dissolve 3,40 g of potassium dihydrogen phosphate (KH2P04) and 3,55 g of disodium hydrogen phosphate
(Na2HP04) in water and make up to 1 000 cm3 in a volumetric flask.
The pH of this solution is 6,87 at 23 °C.
Store the solution in a glass or polyethylene vessel, which is resistant to chemicals.

3.2 Buffer solution, of pH 4.

Dissolve 10,21 g of potassium hydrogen phthalate (KOOC C6H4 COOH) in water and make up to 1 000 cm3
in a volumetric flask.
The pH of this solution is 4,00 at 23 °C.
Store the solution in a glass or polyethylene vessel, which is resistant to chemicals.

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ISO 976:2013(E)


3.3 Buffer solution, of nominal pH 9

Dissolve 3,814 g of sodium tetraborate decahydrate (Na2B4O7 10H2O) in water and make up to 1 000 cm3
in a volumetric flask.
The pH of this solution, when freshly prepared, is 9,20 at 23 °C.
Store the solution in a glass or polyethylene vessel, which is resistant to chemicals, and fitted with a
soda-lime carbon dioxide trap. Replace the solution after one month.
Alkaline buffer solutions are unstable; they absorb carbon dioxide from the atmosphere. When an alkaline
buffer has been used for calibration, the accuracy can be verified by means of the buffer solution of pH 4.

3.4 Reference electrolyte.

Use 3 mol/dm3 potassium chloride solution saturated with silver chloride.

4 Apparatus
Use usual laboratory equipment and the following.

4.1 pH-meter, with an input impedance of at least 1012 Q, a resolution of 0,01 pH units and equipped
for temperature compensation.

4.2 Combined electrode, in which the glass electrode is surrounded concentrically by the silver
reference electrode. The reference electrolyte (3.4) is kept in electrical contact with the test sample by
a chemically inert diaphragm, e.g. a retractable sleeve made of polytetrafluoroethylene or glass. This is
supplied with the electrode by the electrode manufacturer.

A typical combined electrode is shown in Figure 1.

The glass electrode used shall be one recommended by the manufacturer as suitable over the pH range
to be encountered (0 to 14 in the case of polychloroprene latices).
Electrical contact between the electrolyte and the test sample is maintained through a thin film of
electrolyte between the sleeve and the electrode.
The electrode functions linearly between pH 0 and the appearance of the alkaline error, which, depending
on the sodium ion concentration, usually does not appear until the pH is over 11.

4.3 Magnetic stirrer and magnetic bar.

4.4 Electrode holder.

5 Sampling
Carry out the sampling of the rubber latex or polymer dispersion in accordance with one of the methods
specified in ISO 123 or ISO 15528.

6 Procedure

6.1 General
In order to reduce thermal and electrical hysteresis effects, ensure that the temperatures of the test
samples, electrode, demineralized or distilled rinsing water and buffer solutions are as close to one

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ISO 976:2013(E)


another as possible. The temperatures of the test samples and buffer solutions shall not differ by more
than 1 °C. The temperature for the determination shall be 23 °C ± 3 °C (27 °C ± 3 °C in tropical countries).
NOTE The pH variation over the range of 20 °C to 30 °C is negligible. In addition, the temperature compensator
in the instrument should be set at the actual temperature.

6.2 Maintenance of the electrode

The combined electrode (4.2) shall be maintained following the manufacturer’s instructions, paying
particular attention to the following points.
a) Refill the electrode with the reference electrolyte (3.4) through the filling hole, first removing
the filling cap if one is fitted. Slightly withdraw the seated sleeve to eliminate any latex deposits
and allow a drop of the electrolyte to appear before reseating the sleeve. Prior to calibration and
measurement, remove the cap on the electrolyte filling hole to allow the reference electrolyte to be
at atmospheric pressure.
b) When it is not in use, keep the electrode with the junction immersed in the electrolyte.

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ISO 976:2013(E)


Key
1 sliding head 6 reference electrolyte (3.4)
2 filling hole 7 seated PTFE or glass diaphragm (sleeve)
3 connector 8 internal buffer
4 reference electrode 9 membrane
5 internal electrode

Figure 1 — Typical combined electrode

6.3 Calibration of the pH-meter

6.3.1 Switch on the pH-meter (4.1) and allow the electronic circuit to stabilize. Calibrate the pH-meter
following the manufacturer’s instructions. If not available, proceed as follows.

6.3.2 Select two commercial buffer solutions (see Clause 3), one of nominal pH 7 (i.e. close to the zero
point of the electrode) and the other differing from the first by about 3 pH units and of a higher or lower pH
corresponding to the sample to be tested. In the event that commercial buffer solutions are not available,
use the appropriate prepared buffer solutions (3.1 and 3.2 or 3.3).

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